WO2020110941A1 - Composition de caoutchouc pour pneumatique - Google Patents

Composition de caoutchouc pour pneumatique Download PDF

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Publication number
WO2020110941A1
WO2020110941A1 PCT/JP2019/045803 JP2019045803W WO2020110941A1 WO 2020110941 A1 WO2020110941 A1 WO 2020110941A1 JP 2019045803 W JP2019045803 W JP 2019045803W WO 2020110941 A1 WO2020110941 A1 WO 2020110941A1
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Prior art keywords
mass
rubber
parts
tire
rubber composition
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PCT/JP2019/045803
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English (en)
Japanese (ja)
Inventor
克典 清水
誠人 尾崎
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横浜ゴム株式会社
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Application filed by 横浜ゴム株式会社 filed Critical 横浜ゴム株式会社
Priority to EP19891438.4A priority Critical patent/EP3888939A4/fr
Priority to JP2020557667A priority patent/JP7103434B2/ja
Priority to CN201980069390.9A priority patent/CN112867608B/zh
Publication of WO2020110941A1 publication Critical patent/WO2020110941A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • B60C1/0016—Compositions of the tread
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L15/00—Compositions of rubber derivatives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00—Compositions of natural rubber

Definitions

  • the present invention mainly relates to a rubber composition for a tire intended to be used for an undertread portion of a pneumatic tire.
  • tan ⁇ at 60° C. (hereinafter, referred to as “tan ⁇ (60° C.)”) measured by dynamic viscoelasticity is generally used, and tan ⁇ (60° C.) of the rubber composition is small. The lower the exothermicity, the less. Then, as a method of reducing tan ⁇ (60° C.) of the rubber composition, for example, it is possible to reduce the compounding amount of a filler such as carbon black or increase the particle size of carbon black. Alternatively, it has been proposed to blend silica (see, for example, Patent Document 1).
  • the object of the present invention is a rubber composition for a tire intended mainly for use in the undertread portion of a pneumatic tire, which has low rolling resistance, and is excellent in steering stability and durability when formed into a tire. To provide a rubber composition for a tire.
  • the rubber composition for a tire of the present invention which achieves the above object, contains carbon black and silica in 100 parts by mass of a rubber component containing 50% by mass or more of natural rubber and 15% by mass to 50% by mass of terminal-modified butadiene rubber.
  • the elastic modulus is 60% or more.
  • the rubber composition for tires of the present invention uses a terminal modified butadiene rubber in addition to natural rubber as a rubber component, and uses carbon black and silica as a filler in combination, and the hardness and impact resilience of the rubber composition are as described above.
  • the rolling resistance is reduced, it is possible to improve the steering stability and durability when the tire is used.
  • the compounding amount of silica relative to the total amount of carbon black and silica is set as described above while using the carbon black and silica in combination with the terminal-modified butadiene rubber, it is possible to effectively prevent heat generation without deteriorating heat generation. It is possible to improve steering stability and durability when used as a tire and improve these performances in a well-balanced manner.
  • the “hardness” is the hardness of the rubber composition measured by the durometer type A at a temperature of 20° C. according to JIS K6253.
  • the “repulsion elastic modulus at 40° C.” is the repulsive elastic modulus of the rubber composition measured at a temperature of 40° C. by a Lupke type repulsion elasticity testing device according to JIS K6255.
  • the molecular weight distribution (Mw/Mn) obtained from the weight average molecular weight (Mw) and the number average molecular weight (Mn) of the terminal-modified butadiene rubber is preferably 2.0 or less.
  • the rubber physical properties become better, and it is advantageous to reduce the rolling resistance and to improve the steering stability and durability of the tire.
  • the "weight average molecular weight Mw" and the "number average molecular weight Mn” are measured by gel permeation chromatography (GPC) in terms of standard polystyrene.
  • the terminal functional group of the terminal-modified butadiene rubber is at least one of a hydroxyl group, an amino group, an alkoxyl group, and an epoxy group.
  • the affinity with carbon black and silica is increased, and the dispersibility of carbon black and silica is further improved, so it is possible to more effectively increase the rubber hardness and adhesiveness while maintaining low exothermicity, It is advantageous to balance these performances in a good balance.
  • the blending amount of the filler is 100 parts by mass or more with respect to 100 parts by mass of the rubber component.
  • the amine anti-aging agent it is preferable to add 1.0 to 4.0 parts by mass of the amine anti-aging agent to 100 parts by mass of the rubber component. Further, it is preferable to add more than 0 parts by mass and 2.0 parts by mass or less of wax to 100 parts by mass of the rubber component. By thus blending the antioxidant and wax, the crack resistance and workability can be improved.
  • the rubber composition for a tire of the present invention is preferably used in the undertread portion of a pneumatic tire, and a pneumatic tire using the rubber composition for a tire of the present invention in the undertread portion has steering stability and durability. It is possible to improve fuel efficiency while maintaining good performance.
  • the rubber component is a diene rubber, which always contains natural rubber and terminal-modified butadiene rubber.
  • the natural rubber a rubber normally used in a rubber composition for tires can be used. By blending natural rubber, it is possible to obtain sufficient rubber strength as a rubber composition for tires.
  • the content of the natural rubber is 50% by mass or more, preferably 50% by mass to 85% by mass, more preferably 60% by mass to 85% by mass. If the content of natural rubber is less than 50% by mass, the rubber strength will decrease.
  • the terminal-modified butadiene rubber is a butadiene rubber modified with an organic compound having a functional group at one or both ends of the molecular chain.
  • Examples of the functional group that modifies the terminal of the molecular chain include an alkoxysilyl group, a hydroxyl group (hydroxyl group), an aldehyde group, a carboxyl group, an amino group, an amide group, an imino group, an alkoxyl group, an epoxy group, an amide group, a thiol group, Examples thereof include ether groups and siloxane bonding groups. Among them, at least one selected from a hydroxyl group (hydroxyl group), an amino group, an amide group, an alkoxyl group, an epoxy group, and a siloxane bonding group is preferable.
  • the siloxane bonding group is a functional group having a —O—Si—O— structure.
  • the compounding amount of the terminal-modified butadiene rubber is 15% by mass to 50% by mass, preferably 30% by mass to 40% by mass. If the compounding amount of the terminal-modified butadiene rubber is less than 15% by mass, fuel economy is deteriorated. If the compounding amount of the terminal-modified butadiene rubber exceeds 50% by mass, the rubber strength will decrease.
  • the molecular weight distribution (Mw/Mn) of the terminal-modified butadiene rubber is preferably 2.0 or less, more preferably 1.1 to 1.6. In this way, by using a terminal-modified butadiene rubber with a narrow molecular weight distribution, the rubber physical properties become better, and rolling resistance is reduced while effectively improving steering stability and durability when used as a tire. can do.
  • Mw/Mn molecular weight distribution of the terminal-modified butadiene rubber exceeds 2.0, the hysteresis loss becomes large, the heat generation property of the rubber becomes large, and the compression set resistance decreases.
  • the glass transition temperature Tg of the terminal-modified butadiene rubber used in the present invention is preferably ⁇ 85° C. or lower, more preferably ⁇ 90° C. to ⁇ 100° C. By setting the glass transition temperature Tg in this way, heat generation can be effectively reduced. When the glass transition temperature Tg exceeds ⁇ 80° C., the effect of reducing heat generation cannot be sufficiently obtained.
  • the glass transition temperature Tg of natural rubber is not particularly limited, but can be set to, for example, ⁇ 70° C. to ⁇ 80° C.
  • the terminal-modified butadiene rubber used in the present invention has a vinyl content of preferably 0.1% by mass to 20% by mass, more preferably 0.1% by mass to 15% by mass.
  • the vinyl content of the terminal-modified butadiene rubber is less than 0.1% by mass, the affinity with carbon black or silica is insufficient and it becomes difficult to sufficiently reduce heat generation.
  • the vinyl content of the terminal-modified butadiene rubber exceeds 20% by mass, the glass transition temperature Tg of the rubber composition rises, and rolling resistance and abrasion resistance cannot be sufficiently improved.
  • the vinyl unit content of the terminal-modified butadiene rubber is to be measured by infrared spectroscopic analysis (Hampton method).
  • the increase/decrease in the vinyl unit content in the terminal-modified butadiene rubber can be appropriately adjusted by a usual method such as a catalyst.
  • the tire rubber composition of the present invention may contain a diene rubber other than natural rubber and terminal-modified butadiene rubber.
  • diene rubbers include, for example, butadiene rubber without terminal modification, styrene butadiene rubber, isoprene rubber, acrylonitrile-butadiene rubber and the like. These diene rubbers can be used alone or as an arbitrary blend.
  • the tire rubber composition of the present invention always contains both carbon black and silica as a filler.
  • these fillers are added so that the mass ratio of silica to the total amount of carbon black and silica is 0.1 to 0.5, preferably 0.15 to 0.3. If the mass ratio of silica deviates from this range, the effect of enhancing rubber hardness and adhesiveness while maintaining low exothermicity cannot be obtained. In particular, if the mass ratio of silica is too large, the adhesiveness of the rubber composition may decrease, and the durability of the tire may deteriorate.
  • the compounding amount of the filler containing carbon black and silica is not particularly limited as long as the above mass ratio is satisfied, but the compounding amount of the filler is preferably 55 parts by mass with respect to 100 parts by mass of the above-mentioned diene rubber. It is preferable that the amount is not less than 70 parts by mass, more preferably 70 parts by mass to 90 parts by mass. When the blending amount of the filler is less than 55 parts by mass, the hardness of the rubber composition is lowered. From the relationship between the blending amount of the filler and the mass ratio of silica, the blending amount of silica is preferably 20 parts by mass to 50 parts by mass, more preferably 20 parts by mass to 100 parts by mass of the diene rubber.
  • the amount of carbon black is 40 parts by mass, and the content of carbon black is preferably 30 parts by mass to 60 parts by mass, more preferably 35 parts by mass to 50 parts by mass, relative to 100 parts by mass of the diene rubber.
  • the carbon black used in the present invention preferably has a nitrogen adsorption specific surface area N 2 SA of 140 m 2 /g or less, more preferably 100 m 2 /g to 130 m 2 /g.
  • N 2 SA nitrogen adsorption specific surface area
  • the silica used in the present invention preferably has a CTAB adsorption specific surface area of 140 m 2 /g to 250 m 2 /g, more preferably 150 m 2 /g to 220 m 2 /g.
  • the heat generation property can be improved by using such silica. If the CTAB adsorption specific surface area of silica is less than 130 m 2 /g, the rubber strength will decrease. When the CTAB adsorption specific surface area of silica exceeds 250 m 2 /g, the heat generation property deteriorates.
  • the CTAB adsorption specific surface area of silica shall be measured in accordance with ISO 5794.
  • silane coupling agent When using silica in this way, it is preferable to use a silane coupling agent together.
  • the content of the silane coupling agent is preferably 5% by mass to 10% by mass, more preferably 7% by mass to 9% by mass, based on the mass of silica.
  • silane coupling agent When the blending amount of the silane coupling agent exceeds 10% by mass of the mass of silica, the silane coupling agents are condensed with each other, and the desired effect cannot be obtained.
  • the type of silane coupling agent is not particularly limited, but a sulfur-containing silane coupling agent is preferable, and examples thereof include bis-(3-triethoxysilylpropyl)tetrasulfide, bis(3-triethoxysilylpropyl)disulfide, and 3-trisilane.
  • Examples thereof include methoxysilylpropyl benzothiazole tetrasulfide, ⁇ -mercaptopropyltriethoxysilane, and 3-octanoylthiopropyltriethoxysilane.
  • the rubber composition of the present invention may contain an inorganic filler other than the above-mentioned carbon black and silica.
  • inorganic fillers include clay, talc, calcium carbonate, mica, aluminum hydroxide and the like.
  • an amine anti-aging agent and/or wax By compounding these, crack resistance and workability can be improved.
  • the compounding amount of the amine anti-aging agent is preferably 1.0 part by mass to 4.0 parts by mass, and more preferably 1.5 parts by mass to 3.5 parts by mass with respect to 100 parts by mass of the rubber component.
  • the blending amount of the wax is preferably more than 0 parts by mass and 2.0 parts by mass or less, more preferably 0.1 parts by mass or more and 2.0 parts by mass or less with respect to 100 parts by mass of the rubber component.
  • the amine anti-aging agent and the wax may be blended alone or in combination.
  • the amount of the amine-based antioxidant is less than 1.0 part by mass, the effect of improving the crack resistance and workability cannot be expected, and especially the crack resistance is lowered. If the compounding amount of the amine anti-aging agent exceeds 4.0 parts by mass, the workability is deteriorated. If the amount of the wax compounded exceeds 2.0 parts by mass, the processability will decrease.
  • compounding agents may be added to the rubber composition for tires of the present invention.
  • compounding agents vulcanization or cross-linking agents, vulcanization accelerators, anti-aging agents other than amines, liquid polymers, thermosetting resins, thermoplastic resins and the like, which are generally used for pneumatic tires.
  • a compounding agent can be illustrated.
  • the compounding amount of these compounding agents may be a conventional general compounding amount as long as the object of the present invention is not violated.
  • kneading machine a usual kneading machine for rubber, for example, Banbury mixer, kneader, roll or the like can be used.
  • the hardness of the rubber composition for a tire of the present invention having such a composition is 73 or more, preferably 75 to 80, more preferably 76 to 78.
  • the impact resilience at 40° C. of the rubber composition for tires of the present invention is 60% or more, preferably 60% to 65%, more preferably 62% to 65%. Since the rubber composition of the present invention has such physical properties, it is possible to improve rolling stability and durability of the tire while reducing rolling resistance.
  • the hardness is less than 73, the steering stability when used as a tire is deteriorated.
  • the impact resilience is less than 60%, heat generation is deteriorated and the rolling resistance cannot be reduced.
  • the hardness and the impact resilience are not determined only by the above-mentioned composition, but are physical properties that can be adjusted by the kneading conditions and the kneading method.
  • the rubber composition for a tire of the present invention can improve rolling stability and durability when being made into a tire while reducing rolling resistance due to the above-mentioned composition and physical properties.
  • a terminal modified butadiene rubber is used together, and as a filler, carbon black and silica are used together in an appropriate mass ratio, and these fillers are combined with the terminal modified butadiene rubber.
  • carbon black and silica are used together in an appropriate mass ratio, and these fillers are combined with the terminal modified butadiene rubber.
  • the hardness and impact resilience of the rubber composition are sufficiently increased as described above, it is possible to improve the steering stability and durability of the tire while reducing rolling resistance. Therefore, these performances can be improved in a well-balanced manner.
  • the rubber composition for a tire of the present invention is preferably used in the undertread portion of a pneumatic tire, and the pneumatic tire using the rubber composition for a tire of the present invention in the undertread portion has steering stability and durability. Fuel economy performance can be improved while maintaining good performance.
  • the hardness of the rubber composition was measured at a temperature of 20° C. by a durometer type A according to JIS K6253. Further, the impact resilience of the rubber composition was measured at a temperature of 40° C. by a Lupke impact resilience tester in accordance with JIS K6255.
  • the obtained rubber composition was evaluated for fuel efficiency, steering stability, durability, crack resistance, and workability by the methods shown below.
  • a test tire (tire size 215/45R17) using the obtained rubber composition as an undertread was prepared and mounted on a standard rim (rim size 7JJ) to an air pressure of 230 kPa and an indoor drum tester (drum diameter). : 1707 mm) and rolling at a speed of 80 km/h while being pressed against the drum under a load equivalent to 85% of the maximum load under the air pressure described in JATMA Yearbook 2009 The resistance was measured. The evaluation result was shown by an index with the value of Standard Example 1 being 100, using the reciprocal of the measured value. The larger the index value, the smaller the rolling resistance and the better the fuel economy performance.
  • a test driver conducted a sensory evaluation on the road surface responsiveness when changing the lane at the time of running and traveling 80 km/h on a test course consisting of a paved road surface. The evaluation results are shown by index values with the standard example 1 being 100. The larger this index value, the better the road surface response at the time of lane change, and the better the steering stability.
  • Durability A test tire (tire size 215/45R17) in which the obtained rubber composition was used as an undertread was prepared, mounted on a standard rim (rim size 7JJ), the air pressure was set to 230 kPa, and mounted on a test vehicle of displacement 2000 cc. Then, the car was run on an 8-shaped turning test course under conditions of a turning acceleration of 0.8 G and 500 laps, and the amount of wear of the tread portion after running was measured. The evaluation results are shown by an index with the standard example 1 being 100, using the reciprocal of the measured value. The larger the index value, the smaller the amount of wear and the more excellent the durability.
  • the obtained rubber composition was extruded into a sheet, and two extrudates (sample for crimping) 3 hours after the extruding were subjected to a crimping load of 0.98 N, a crimping time of 0 seconds, and a crimping speed of 50 cm/min. After press-bonding under the conditions, the film was peeled under the condition of a peeling speed of 125 cm/min, and the adhesive force at that time was measured by a PICMA type tack meter (manufactured by Toyo Seiki Seisaku-sho, Ltd.). The evaluation results are shown in AC below.
  • the "tack index” used for the evaluation of A to C is an index with the measured value as standard example 1 being 100.
  • Tables 1 to 3 The types of raw materials used in Tables 1 to 3 are shown below.
  • -NR natural rubber
  • TSR20 glass transition temperature Tg: -65°C
  • SBR styrene butadiene rubber
  • Nipol 1502 glass transition temperature: -60°C
  • -Modified S-SBR Terminal-modified solution-polymerized styrene-butadiene rubber
  • Nipol NS612 manufactured by Nippon Zeon Co., Ltd.
  • BR butadiene rubber
  • Nipol BR1220 manufactured by Zeon Corporation (glass transition temperature Tg: -105°C)
  • -Modified BR1 end-modified butadiene rubber
  • JSR BR54 glass transition temperature Tg: -107°C, functional group: silanol group, molecular weight distribution 2.5
  • Modified BR2 terminal modified butadiene rubber synthesized by the following method (glass transition temperature Tg: -93°C, functional group: polyorganosiloxane group)
  • BR3 end-modified butadiene rubber, Nipol BR1250H manufactured by Nippon Zeon Co., Ltd.
  • CB1 carbon black, Niteron #300IH manufactured by Shin Nikka Carbon Co., Ltd. (nitrogen adsorption specific surface area N 2 SA: 115 m 2 /g)
  • CB2 Carbon black, Niteron #430 (Nitrogen adsorption specific surface area N 2 SA: 134 m 2 /g) manufactured by Shin Nihon Carbon Co., Ltd.
  • Silica 1 Ultrasil VN3 manufactured by Degussa (CTAB adsorption specific surface area: 153 m 2 /g)
  • Silica 2 Zehosil Premier 200MP (CTAB adsorption specific surface area: 210 m 2 /g) manufactured by Rhodia.
  • ⁇ Silane coupling agent Si69 manufactured by Evonik Degussa ⁇ Zinc oxide: Three types of zinc oxide manufactured by Shodo Chemical Industry ⁇ Stearic acid: Lunac S-25 manufactured by Kao -Anti-aging agent 1: amine-based anti-aging agent, Santoflex 6PPD manufactured by Flexis -Anti-aging agent 2: amine-ketone type anti-aging agent, Nocrac 224 manufactured by Ouchi Shinko Chemical Industry Co., Ltd. ⁇ Wax: Ouchi Shinko Chemical Co., Ltd. Sannok Sulfur: Shikoku Kasei Co., Ltd. Mucron OT-20 ⁇ Vulcanization accelerator: Nocceller CZ manufactured by Ouchi Shinko Chemical Industry Co., Ltd.
  • the maximum temperature during the polymerization reaction was 80°C. After the continuous addition was completed, the polymerization reaction was continued for another 15 minutes, and after confirming that the polymerization conversion rate was in the range of 95% to 100%, a small amount of the polymerization solution was sampled. A small amount of the sampled polymerization solution was quenched by adding excess methanol and then air-dried to obtain a polymer, which was used as a sample for gel permeation chromatography (GPC) analysis. Using the sample, the peak top molecular weight and the molecular weight distribution of the polymer (corresponding to a conjugated diene-based polymer chain having an active end) were measured and found to be "230,000" and "1.04", respectively.
  • GPC gel permeation chromatography
  • the styrene-butadiene rubber was blended in place of the terminal-modified butadiene rubber, so the fuel economy performance deteriorated.
  • the rubber composition (tire) of Comparative Example 2 contained the end-modified solution-polymerized styrene-butadiene rubber in place of the end-modified butadiene rubber, and thus had poor fuel economy performance and durability.
  • the rubber composition (tire) of Comparative Example 3 was poor in durability because the compounding amount of the terminal-modified butadiene rubber was too small.
  • silica since silica was not mixed, the fuel economy performance and durability were deteriorated.
  • the rubber composition (tire) of Comparative Example 5 had too low a hardness, and thus had poor steering stability and durability.
  • the rubber composition (tire) of Comparative Example 6 had a too small impact resilience, and thus the heat buildup deteriorated.
  • the rubber composition (tire) of Comparative Example 7 contained not only natural rubber and terminal-modified butadiene rubber but also styrene-butadiene rubber, and thus the durability was deteriorated. Since the rubber composition (tire) of Comparative Example 8 does not contain the terminal-modified butadiene rubber, it is not possible to obtain the effect of improving the fuel economy performance and steering stability performance. Therefore, the crack resistance and durability deteriorated.

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

L'invention concerne une composition de caoutchouc pour pneumatiques qui est destinée principalement à être utilisée dans la production de la partie d'épaisseur sous sculpture d'un pneumatique et qui permet d'obtenir des pneumatiques ayant une faible résistance au roulement et d'excellentes propriétés en termes de stabilité de direction et de durabilité. Des charges comprenant du noir de carbone et de la silice sont incorporées dans 100 parties en masse d'un ingrédient de caoutchouc comprenant au moins 50 % en masse de caoutchouc naturel et 15 à 50 % en masse de caoutchouc de butadiène modifié par un groupe terminal, le rapport en masse entre la quantité de silice incorporée et la quantité de charges incorporées étant de 0,1 à 0,5. Cette composition de caoutchouc est conçue pour avoir une dureté égale ou supérieure à 73 et une résilience à 40 °C égale ou supérieure à 60 %.
PCT/JP2019/045803 2018-11-30 2019-11-22 Composition de caoutchouc pour pneumatique WO2020110941A1 (fr)

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EP19891438.4A EP3888939A4 (fr) 2018-11-30 2019-11-22 Composition de caoutchouc pour pneumatique
JP2020557667A JP7103434B2 (ja) 2018-11-30 2019-11-22 空気入りタイヤ
CN201980069390.9A CN112867608B (zh) 2018-11-30 2019-11-22 轮胎用橡胶组合物

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WO2023190688A1 (fr) * 2022-03-31 2023-10-05 横浜ゴム株式会社 Composition de caoutchouc pour pneus

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023190688A1 (fr) * 2022-03-31 2023-10-05 横浜ゴム株式会社 Composition de caoutchouc pour pneus
JP7473825B2 (ja) 2022-03-31 2024-04-24 横浜ゴム株式会社 タイヤ用ゴム組成物

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Publication number Publication date
JP7103434B2 (ja) 2022-07-20
EP3888939A4 (fr) 2022-07-27
JPWO2020110941A1 (ja) 2021-10-07
EP3888939A1 (fr) 2021-10-06
CN112867608A (zh) 2021-05-28
CN112867608B (zh) 2022-05-17

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